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Nguyen Vu Son WEO

ID: USTHBI5-118
Experiment Date: 07/10/2016

Lab Report

Separation and Purification of


Inorganic Compounds by Ionexchange Chromatography
1.Introduction
Nowadays, the worlds water supply is prone to various contaminants such as
heavy metals that are able to cause tremendously bad influences on the human
body. Hence, the urge to purify such contaminants from water is becoming of great
importance worldwide (Atamanenko & Kornilovich , 2001). In this experiment, we
examined the capability of the ion-exchange chromatography to separate ions of
two heavy metals, copper (II) and cadmium (II), from water and therefor to act as a
purification method. The additional objective of our experiment is to investigate the
implementation of ion-exchange chromatography in laboratorial scale to separate
two metals from a solution.
Ion-exchange chromatography is based on the covalent bonding of ions on the
stationary solid phase, usually a resin. Resins are amorphous, or non-crystal,
particles of organic material that have a negatively charged surface (cation
exchangers), on which cations are attracted, or a positively charged surface
(anion exchangers) (Harris, 2010). For this experiment, the anion exchanger KY-23
in hydrogen form was used to capture copper (II) and cadmium (II) in the mobile
phase, which is a solution. As the metal ions are carried through the column of resin
beads, they are exchanged for the hydrogen atoms readily bonded to the resin
beads surface. As a result, metals ions are adsorbed on the resin beads surface
while H+ ions enter the fluid stream and are present in the washing water. The
process can be reverse by a solution of acid by the same mechanism in order to
regenerate the resin beads for future use.

2.Description of the method


2.1
-

Equipment and Materials


50ml burette.
100ml and 500ml beaker.
Glass rod.
KY-23 resin beads in the hydrogen form.
Cotton fiber.
Abundant demineralized water.

10 ml Cd ( NO 3 )2 0.5 M nCd ( NO ) =n Cd ( NO ) .4 H O=0.5 0.01=0.005 mole


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mCd ( NO ) .4 H O =1.542 g .
3 2

10 ml CuS O4 0.5 M nCuS O =nCuSO


4

mCuS O

.5 H2 O

.5 H2 O

Actual amount used: 1.543g

=0.5 0.01=0.005 mole

=1.25 g . Actual amount used: 12.5g

Mixture of 5ml glycerol and 5g NaOH in 100ml distilled water.


5% solution of hydrochloric acid.
Sodium sulfide solution.

2.2 Procedure
1. A small chunk of cotton fiber was stacked into the burette and pushed down
the tube using distilled water. Later, the resin beads were stacked not too
tightly into the burette, bringing the cotton further down to the small neck of
the burette. The total height of the resin column was set to be 30cm and the
burette was filled with distilled water and had to remain always above the
resin level.
2. The adjustment valve of the burette was adjusted to yield an eluent flow rate
of roughly 5ml/minute. After obtaining the desired flow rate, the valve was
not to be touched throughout the experiment.
3. Two 100ml solutions of cadmium nitrate and copper sulfate were prepared for
9 groups, each group took 10ml of each solution and create a mixture.
4. A 100ml beaker was positioned to capture the effluent and then the mixture
was poured down the burette. The collected washing water in the beaker was
then checked for the presence of copper ions using color and cadmium ion
using some drops of sodium sulfide.
5. The 105ml mixture of glycerol and sodium hydroxide was then poured down
the burette to desorb cooper ions. As soon as the outlet showed some blue
color, a 500ml beaker was set to collect the blue solution of copper ions. After
the blue color disappeared from the outlet, 50ml of distilled water was poured
in.
6. The 500ml beaker containing blue copper solution was then replaced by a
new 500ml beaker. Afterward, 50ml of 3% HCl solution was poured down the
burette to collect cadmium ion.
7. A sodium sulfide solution was used to precipitate all cadmium and cooper
ions in the two 500ml beakers. The precipitates were then screened out using
filter paper, dried at 100 0C and finally used to calculate the yield of each
metal ion.

3. Result and Observation


The mixture of cadmium and cooper ions had a light blue color, however, after
the solution went through the resin column, the collected washing water had no
color. The test using sodium sulfide hardly showed any yellow precipitation (CdS).
When we poured down the mixture of glycerol and sodium hydroxide down the tube,

the solution at the outlet started to turn dark blue. After a while, the color of the
effluent started fading away and after that, we poured in 50ml distilled water. When
the solution in the beaker reach about 150ml, we replaced it with another one and
poured 50ml HCl into the burette. The obtained solution was light blue.
When we added the sodium sulfide into the two beakers, precipitation instantly
occurred in both of them. The precipitates were then filter, dried and weight to be
0.679g for dark blue solution and 0.916g for light blue solution. The theoretical
weights of CuS and CdS are calculated below:

nCd =n Cd ( NO ) =0.005 mole mCdStheoretical =nCd M CdS =0.005 144.4=0.722 g


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nCu =nCuSO =0.005 mole m CuStheoretical =nCu M CuS =0.005 95.5=0.478 g


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4.Discussion
The initial color of the mixture solution was light blue because of the copper
ions. However, after the mixture passed though the resin, the resulting solution had
no color which indicates that copper was fully adsorbed onto the resin bead surface.
Cadmium ion can form a bright yellow precipitate with sulfide ion, S -. Nevertheless,
when the first washing water was tested with sodium sulfide, we observed no yellow
precipitate, thus, all cadmium ions had been retained by the resin. The two
observations above proved the ability of the chosen resin to capture cations in a
solution.
When glycerol and sodium hydroxide entered the resin layer, the outlet turned
blue because of the reaction between copper cations, hydroxyl anions and glycerol
that liberated copper from the resin beads surface into the solution. The equation is:

Source: Wikipedia.
After all the blue solution was collected, we poured in hydrochloric acid with the
intention to use hydrogen ions to replace and release cadmium ions from the resin.
However, the washing water we collected had a light blue color. The reason for this
phenomenon could be the incomplete desorption of copper ions from the previous
step, so that beside cadmium ions, H + also released the remaining copper and
created light blue solution. In order to explain the incomplete desorption, there are
two possible reasons. First, the resin column was not correctly packed so that there
was some air inside, thus, reduce the efficiency. Second, the amount of glycerol and
hydroxyl utilized was not enough to release all copper into the solution.
Regarding the dark blue solution, it is undoubtedly that it contained only copper
ions since only copper has the reaction with glycerol, thus, all the precipitate from
this solution was copper sulfide only. Since the light blue solution contained both
cadmium and copper ions, it is hard to distinguish from the precipitates how much

grams was of cadmium sulfide and how much grams was of copper sulfide. In that
case, we assumed that hydrochloric acid must had released all the cadmium and
the remaining copper ions, and the weight of cadmium sulfide is equal to the
theoretical weight of 0.722g and the copper sulfide was 0.194g. Hence, we had the
total weight of CdS and CuS obtained were 0.722g and 0.873g, respectively.
However, the theoretical weight of CuS was only 0.478g, which is only about half
the value obtained. From the outset, only copper and cadmium ions were added
that can form precipitate with sulfide anions, hence, the only plausible explanation
is that there was an interference that also precipitated with sulfide. In this
experiment, only the resin beads were not controlled by us and they are the most
likely source of interference. Moreover, the resin was previously used for the same
experiment and therefore some cadmium and copper could have left due to poor
regeneration. If this was the case, both the values of CdS and CuS would be bias
and the recovery of such ions in this experiment would be a failure.

5.Conclusion
Our experiment has succeeded in proving the ability of the ion-exchange
chromatography to retain the heavy metals ions, in other word, to purify such ions
from water. Nevertheless, the experiment was only in the laboratory scale, so the
application of the method in large scale still require further studies. Additionally, we
were able to verify the operation of the chromatography method in analytical
separation. However, since the result was so bias and there was some interferences
in the process, we were unable to examine the efficiency of the separation method.

6.References
Atamanenko , I., & Kornilovich , B. (2001, October). A role of the clay minerals in the
membrane purification. Separation and Purication Technology, 25(1-3), 487492. doi:10.1016/S1383-5866(01)00078-8
Harris, D. C. (2010). Quantitative Chemical Analysis (8th ed., Vol. 25). W. H.
Freeman.

7.Declaration
This lab report is my own work. I understand the requirements for academic honesty. I am
aware of plagiarism and its penalties. I have not re-used previously submitted material in this
report. I have not engaged someone else to complete this report. I have retained a duplicate hard
copy of this report.
Student Signature:

Date: 11/10/2016.